参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | (3S)-(-)-3-(二甲氨基)吡咯烷 | HCID 7019156 | — |
| 反应物 | 2-溴-4-氯苯腈 | HCID 23498524 | — |
| 试剂 | 碳酸氢铯 | HCID 10796 | — |
| 催化剂 | 1,1'-联萘-2,2'-双二苯膦 (BINAP) | HCID 634876 | — |
| 催化剂 | 三(二亚苄基丙酮)二钯 | HCID 9811564 | — |
| 溶剂 | 甲苯 | HCID 1140 | — |
| 产物 | 4-chloro-2-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]benzonitrile | HCID 178418212 | 69.34% |
反应步骤
A mixture of 2-bromo-4-chlorobenzonitrile (500 mg, 2.31 mmol), (S)-N,N-dimethylpyrrolidin-3-amine (317 mg, 2.77 mmol), cesium carbonate (1505 mg, 4.62 mmol), tris(dibenzylideneacetone)dipalladium(0) (212 mg, 0.23 mmol) and BINAP (288 mg, 0.46 mmol) in toluene (15 mL) was stirred at 100 °C for overnight. Conc. in vacuo, the residue was purified with ISCO (100% ethyl acetate to 30% methanol in ethyl acetate) to yield a light yellow solid as (S)-4-chloro-2-(3-(dimethylamino)pyrrolidin-1-yl)benzonitrile (400 mg, 69.3 %).
来源与证据
| 来源数据集 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-58bee23c6bfd4e46abec561eea6c720a |
|---|
| 来源说明 | 750 AstraZeneca ELN dataset |
|---|
